微波辅助萃取-衍生气相色谱-电子捕获检测器法测定电子电气产品中的四溴双酚A

以N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA)作衍生化试剂,采用微波辅助萃取-衍生气相色谱-电子捕获检测器法(GC-ECD)测定电子电气产品中的四溴双酚A。使用V(甲苯)∶V(甲醇)=10∶1微波辅助萃取电子电气样品,用正己烷沉淀萃取液中的高聚物,净化后,将萃取液进行衍生化反应,采用ECD检测器进行定量测定。对衍生化时间、衍生化温度、衍生化试剂用量、沉淀试剂用量等前处理条件进行了优化,并进行了线性、回收率、精密度等试验。结果表明,方法线性范围为0.005~5 mg/L,相关系数为0.9985,方法的检测下限为0.02 mg/kg。采用样品加标的方式进行四溴双酚A的精密度及回收率实验,回收率在81.7%~110%之间,相对标准偏差RSD(n=7)小于7.2%。所建方法能很好的应用于电子电气产品中四溴双酚A的检测。

Determination of tetrabromobisphenol A in electrical and electronic equipment by microwave-assisted extraction-pre-derivatization-gas chromatography with an electron capture detector

A rapid and effective pre-derivatization-gas chromatography coupled with an electron capture detector has been developed systematically and studied for the determination of tetrabromobisphenol A in electrical and electronic equipments, in which N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) was taken as a derivatization reagent. In this study, the sample was extracted with toluence and methanol mixture (10∶1, V/V), and the polymer in the extracting solution was precipitated with n-hexane. After purification, target compounds was derivated with BSTFA. Quantitative analysis was carried out by GC-ECD. Under the optimal derivatization and extraction conditions, such as derivatization time, derivatization temperature, dosage of derivatization reagent and dosage of precipitation reagent et al., good linearity, recovery and precision were obtained. The linear range was from 0.005 mg/L to 5 mg/L with a correlation coefficient of 0.9985. The lowest detection limit of the method was 0.02 mg/kg. The recoveries and RSD were 81.7%～110% and below 7.2% respectively. The established method has been successfully applied to the determination of tetrabromobisphenol A in electrical and electronic equipments.